Copper dibenzyl dithiocarbamate synthesis equipment

Abstract

The utility model discloses copper dibenzyl dithiocarbamate synthesis equipment, and relates to the technical field of breast cancer treatment. Comprising a first stirring container, a second stirring container, a stainless steel high-pressure reaction kettle, a rotary evaporator and a suction flask, a liquid extraction auxiliary structure is arranged between the first stirring container and a Buchner funnel on the suction flask and is used for assisting in guiding a liquid reactant in the first stirring container into the Buchner funnel so as to be matched with the suction flask to carry out reduced pressure filtration operation to generate filtrate; the rotary evaporator is used for carrying out rotary evaporation on the filtrate and separating out solids. The equipment is designed into corresponding synthesis equipment based on the synthesis step of copper dibenzyldithiocarbamate, and a liquid extraction auxiliary structure is added in the complicated manual operation step to assist in transferring a magnetically stirred solution into a Buchner funnel of a suction flask, so that the operation efficiency in the step is accelerated, and the production cost is reduced. Further, the synthesis work efficiency of the copper dibenzyl dithiocarbamate is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to breast cancer treatment technical field especially relates to copper dibenzyl dithiocarbamate synthesis equipment. BACKGROUND

[0002] Breast cancer is the most common female cancer, accounting for about 23% of the total number of cancers, and triple-negative breast cancer is a group of heterogeneous breast cancer; chemotherapy is the only systemic treatment for improving its prognosis, and the main drugs are paclitaxel and anthracycline drugs, but no specific chemotherapy drug has superiority in specific breast cancer phenotype, and even if the tumor has a good response to the chemotherapy drug, it can still be in a rapid progression state. Copper dibenzyl dithiocarbamate is integrated by integrating the chemical groups that can currently treat triple-negative breast cancer, does not need in vivo conversion, and is fixed on breast cancer cells through NPL4 receptors, which is different from the previous cytotoxic drugs and biological agents. After the synthesis of the previous related groups, in vivo conversion is needed to act on breast cancer cells, but copper dibenzyl dithiocarbamate does not need in vivo conversion and directly acts on triple-negative breast cancer cells to treat triple-negative breast cancer, and reduces the treatment cost and serves the patients. The synthesis method of copper dibenzyl dithiocarbamate is as follows: 8ml, N, N-dimethylformamide (DMF), 1mmol (0.295g) sodium dibenzyl dithiocarbamate, 1mmol (0.171g) copper chloride dihydrate and 2ml H2O are added in a beaker, and stirring is carried out to make them all dissolved. The solution is transferred into a 25ml polytetrafluoroethylene lined stainless steel high-pressure reaction kettle, and is reacted at 80℃ for 72 hours. After the reaction is completed, the reaction kettle is cooled to room temperature at a speed of 10℃ / min, and dark green crystals are precipitated on the inner wall of the reaction kettle. The preparation process of sodium dibenzyl dithiocarbamate is as follows: acetonitrile (150ml) is measured in a 250ml round-bottom flask, dibenzylamine 11.8g (0.06moL) is added, stirring is carried out in an ice water bath (0-4℃), carbon disulfide 6.96g (0.09mol) and 4.7ml sodium hydroxide solution (mass fraction 50%) are added, and the reaction is carried out under magnetic stirring for 16 hours, and then filtration is carried out. The filtrate is rotary evaporated to precipitate solid, which is washed with diethyl ether and dried to obtain the product 13.04g. The crude product is recrystallized with acetonitrile to obtain sodium dibenzyl dithiocarbamate 11.1g.

[0003] In the synthesis of copper dibenzyl dithiocarbamate, some conventional operation steps are involved, and conventional experimental equipment in the prior art is used, including magnetic stirring equipment, vacuum filtration operation, a rotary evaporator, a stainless steel high-pressure reaction kettle and the like, but in combination in the operation process, such as the solution transfer operation in the suction filtration operation after magnetic stirring, the solution currently needs to be manually transferred to a Buchner funnel of a suction filter flask, and then subsequent suction filtration operation is performed, so that the process working efficiency is low, and therefore, in combination with the entire step of the synthesis of copper dibenzyl dithiocarbamate, a copper dibenzyl dithiocarbamate synthesis device is designed to improve the convenience of the corresponding operation. Content of the utility model

[0004] The utility model discloses a copper dibenzyl dithiocarbamate synthesis device.

[0005] In order to realize the above-mentioned purpose, the utility model provides the following technical scheme:

[0006] The copper dibenzyl dithiocarbamate synthesis device of the utility model comprises:

[0007] The first stirring container, the second stirring container, the stainless steel high-pressure reaction kettle, the rotary evaporator and the suction filter flask are provided with a Buchner funnel, an auxiliary liquid suction structure is arranged between the first stirring container and the Buchner funnel on the suction filter flask to assist the liquid reactant in the first stirring container to be introduced into the Buchner funnel to cooperate with the suction filter flask to perform vacuum filtration operation to generate filtrate, the rotary evaporator is used to evaporate the filtrate to precipitate solid matter, the second stirring container is used to perform the synthesis reaction of copper dibenzyl dithiocarbamate, and the solution after reaction in the second stirring container is reacted in the stainless steel high-pressure reaction kettle at a temperature of 80 DEG C for 72 hours.

[0008] Further, the reactant in the first stirring container is subjected to magnetic stirring by arranging a magnetic stirrer.

[0009] Further, a safety cock is arranged on the suction filter flask to balance the air pressure in the suction filter flask.

[0010] Further, the suction filter flask is subjected to air suction by an air suction pump to generate negative pressure.

[0011] Further, the liquid pumping auxiliary structure comprises a pipe adapter, first and second pipes are arranged at two ends of the pipe adapter respectively, a fixing clamp structure is arranged at a lower end of the pipe adapter to be fixed at a position of a mouth of the first stirring container, a supporting guide pipe is arranged at one side of the pipe adapter, a pumping pipe is coaxially arranged in the supporting guide pipe, one end of the pumping pipe is connected with the first pipe, the other end of the pumping pipe extends into the supporting guide pipe and slides in the supporting guide pipe, and a lower end of the pumping pipe extends out of a lower end of the supporting guide pipe and into the first stirring container.

[0012] A guide opening is arranged on a side surface of the supporting guide pipe, a slider connected with an outer side surface of one end of the pumping pipe is arranged in the guide opening, the other end of the slider extends out of the supporting guide pipe from the guide opening, the slider slides in the guide opening and drives the pumping pipe to slide in the supporting guide pipe.

[0013] The other end of the second pipe is provided with a docking cover in communication with the second pipe, and a sealing plug is arranged at a distal end of the docking cover and inserted into the Buchner funnel, the sealing plug is sealingly matched with the Buchner funnel at an outer side thereof and is in communication with the docking cover at an inner side thereof.

[0014] Further, the fixing clamp structure comprises a door-shaped frame fixedly connected to a bottom surface of the lower end of the pipe adapter, the door-shaped frame is used to extend a side wall of the mouth of the first stirring container into the door-shaped frame, and a jacking bolt in screwing cooperation with the door-shaped frame is arranged at one side of the door-shaped frame to be jacked on an outer side wall of the first stirring container to fix the door-shaped frame at the position of the mouth of the first stirring container.

[0015] Further, the stainless steel high-pressure reaction kettle is internally provided with a polytetrafluoroethylene lining.

[0016] In the above technical solution, the copper dibenzyl dithiocarbamate synthesis equipment has the following beneficial effects:

[0017] The device is designed into a corresponding synthesis device based on a copper dibenzyl dithiocarbamate synthesis step, and a liquid pumping auxiliary structure is added in a complicated manual operation step to assist in transferring the magnetically stirred solution into the Buchner funnel of the suction filter bottle, so as to accelerate the operation efficiency in this step and improve the copper dibenzyl dithiocarbamate synthesis work efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments will be briefly introduced as follows. Obviously, the drawings in the following description are only some embodiments described in the present application, and other drawings can also be obtained by those skilled in the art according to these drawings.

[0019] Fig. 1 The structural schematic diagram of the copper dibenzyl dithiocarbamate synthesis equipment provided by the embodiment of the present application is shown in the figure.

[0020] Fig. 2 The structural schematic diagram of the liquid pumping auxiliary structure of the copper dibenzyl dithiocarbamate synthesis equipment provided by the embodiment of the present application is shown in the figure.

[0021] Explanation of reference signs:

[0022] 1, first stirring container; 2, second stirring container; 3, stainless steel high-pressure reaction kettle; 4, rotary evaporator; 5, suction filter bottle; 6, Buchner funnel; 7, magnetic stirrer; 8, safety cock; 9, air pump; 10, conduit adapter; 11, first conduit; 12, second conduit; 13, support guide pipe fitting; 14, liquid pumping pipe; 15, guide opening; 16, sliding block; 17, butt joint cover; 18, sealing plug; 19, door-shaped frame; 20, jacking bolt. Specific implementation

[0023] In order to make those skilled in the art better understand the technical solutions of the present application, the present application will be further described in detail in combination with the drawings.

[0024] Please refer to Figs. 1-2 , copper dibenzyl dithiocarbamate synthesis equipment, comprising:

[0025] The first stirring container 1, the second stirring container 2, the stainless steel high-pressure reaction kettle 3, the rotary evaporator 4 and the suction filter bottle 5, wherein the first stirring container 1 and the second stirring container 2 can be conventional open stirring containers, such as flasks, for stirring; the suction filter bottle 5 is provided with a Buchner funnel 6 having a filter paper for filtering; a suction auxiliary structure is arranged between the first stirring container 1 and the Buchner funnel 6 on the suction filter bottle 5 to assist the introduction of the liquid reactant in the first stirring container 1 into the Buchner funnel 6 to cooperate with the suction filter bottle 5 to perform a reduced-pressure filtration operation to generate a filtrate; in this process, the solution prepared in the first stirring container 1 directly passes through the suction auxiliary structure, and when the suction filter bottle 5 is in a working state to generate negative pressure, the solution directly passes through the suction auxiliary structure connected with the Buchner funnel 6, and the suction filter operation is performed while the solution is being extracted, thereby greatly improving the working efficiency of this operation step; the rotary evaporator 4 is used to evaporate the filtrate to separate solid substances; the second stirring container 2 is used to perform a synthesis reaction of copper dibenzyl dithio carbamate; and the solution after the reaction in the second stirring container 2 is reacted in the stainless steel high-pressure reaction kettle 3 at a temperature of 80°C for 72 hours.

[0026] Specifically, acetonitrile (150 ml) is measured in the first stirring container 1, and dibenzylamine 11.8 g (0.06 mol) is added thereto, and the mixture is fully stirred in an ice water bath (0-4°C), and carbon disulfide 6.96 g (0.09 mol) and 4.7 ml of a sodium hydroxide solution (mass fraction 50%) are added thereto, and the mixture is magnetically stirred for 16 hours, and then the suction filter operation is performed on the suction filter bottle 5. The filtrate is evaporated by the rotary evaporator 4 to separate solid substances, which are washed with diethyl ether and dried to obtain the product 13.04 g. The crude product is recrystallized with acetonitrile to obtain sodium dibenzyl dithio carbamate 11.1 g.

[0027] In the second stirring container 2, 8 ml of N,N-dimethylformamide (DMF), 1 mmol (0.295 g) of sodium dibenzyl dithio carbamate, 1 mmol (0.171 g) of copper chloride dihydrate and 2 ml of H2O are added and stirred to dissolve them all. The solution is transferred into a 25 ml stainless steel high-pressure reaction kettle, and reacted at 80°C for 72 hours. After the reaction is completed, the reaction kettle is cooled to room temperature at a speed of 10°C / min, and ink green crystals are separated on the inner wall of the reaction kettle.

[0028] Further, the reactants in the first stirring container 1 are magnetically stirred by the magnetic stirrer 7.

[0029] Further, the safety cock 8 is arranged on the suction filter bottle 5 to balance the air pressure in the suction filter bottle 5. After the suction filter bottle 5 is used, the safety cock 8 is unscrewed to balance the air pressure in the suction filter bottle 5 and the atmosphere outside the suction filter bottle 5, so as to release the working state.

[0030] Further, the suction filter bottle 5 is connected with the air suction pump 9 to generate negative pressure.

[0031] Further, the liquid extraction auxiliary structure comprises a conduit adapter 10, the conduit adapter 10 is provided with a first conduit 11 and a second conduit 12 at both ends, so that the first conduit 11 and the second conduit 12 are connected in communication through the conduit adapter 10, the lower end of the conduit adapter 10 is provided with a fixing clamp structure for fixing the mouth position of the first stirring container 1, one side of the conduit adapter 10 is provided with a supporting guide pipe 13, that is, the conduit adapter 10 and the supporting guide pipe 13 are fixed on the mouth position of the first stirring container 1 through the fixing clamp structure, so as to facilitate the operation of extracting the solution, the supporting guide pipe 13 is coaxially provided with a liquid extraction pipe 14, one end of the liquid extraction pipe 14 is connected with the first conduit 11, the other end of the liquid extraction pipe 14 extends into the supporting guide pipe 13 and slides in the supporting guide pipe 13, the lower end of the liquid extraction pipe 14 extends out of the lower end of the supporting guide pipe 13 and extends into the first stirring container 1;

[0032] The side surface of the supporting guide pipe 13 is provided with a guide opening 15, the guide opening 15 is provided with a sliding block 16 connected to the outer surface of one end of the first conduit 11 on the liquid extraction pipe 14, the other end of the sliding block 16 extends out of the supporting guide pipe 13 from the guide opening 15, the sliding block 16 slides in the guide opening 15 and drives the liquid extraction pipe 14 to slide in the supporting guide pipe 13;

[0033] The other end of the second conduit 12 is provided with a docking cover 17 connected in communication therewith, the docking cover 17 is provided with a sealing plug 18 inserted into the Buchner funnel 6, the outer side of the sealing plug 18 is sealingly connected with the Buchner funnel 6, and the inner side of the sealing plug 18 is connected in communication with the docking cover 17.

[0034] Specifically, after the docking cover 17 is sealingly connected with the Buchner funnel 6 through the sealing plug 18, the docking cover 17 is connected in communication with the Buchner funnel 6, and then the sliding block 16 is pushed to slide in the guide opening 15, thereby driving the liquid extraction pipe 14 to slide in the supporting guide pipe 13, so that the liquid extraction pipe 14 can be moved downward to extend out of the supporting guide pipe 13 and extend into the first stirring container 1, so as to extract the liquid in the first stirring container 1, at this time, the filtration work of the filtration bottle 5 is started, so that the solution is extracted in the first stirring container 1 through the liquid extraction auxiliary structure, and the filtration work is carried out through the filtration bottle 5, which reduces the manual operation and the mistakes caused by the manual operation, and improves the work efficiency of this step.

[0035] Further, the fixed clamp structure comprises a door-shaped frame 19 fixedly connected to the bottom surface of the lower end of the conduit adapter 10, the door-shaped frame 19 is used to extend into the side wall of the mouth position of the first stirring container 1, and a jacking bolt 20 threadedly connected to one side of the door-shaped frame 19 is used to be jacked on the outer side wall surface of the first stirring container 1 to fix the door-shaped frame 19 on the mouth position of the first stirring container 1. The door-shaped frame 19 is equivalent to riding on the mouth of the first stirring container 1 and is fixed by the jacking bolt 20, and the end of the jacking bolt 20 should be fixed with a rubber head to avoid damaging the first stirring container 1.

[0036] Further, the stainless steel high-pressure reaction kettle 3 is internally provided with a polytetrafluoroethylene lining to protect the stainless steel high-pressure reaction kettle 3 and prevent the stainless steel high-pressure reaction kettle 3 from being corroded by chemical reactants.

[0037] In summary, the device is designed as a corresponding synthesis device based on the synthesis steps of copper dibenzyl dithiocarbamate, and an auxiliary liquid pumping structure is added in the complicated manual operation steps to assist in transferring the magnetically stirred solution to the Buchner funnel of the filtration bottle, so as to speed up the operation efficiency in this step, and thus improve the synthesis work efficiency of copper dibenzyl dithiocarbamate.

[0038] The above only describes some exemplary embodiments of the present application by way of illustration, and it is needless to say that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present application. Therefore, the above drawings and descriptions are illustrative in nature and should not be understood as limiting the scope of protection of the present application.

Claims

1. Equipment for synthesizing copper dibenzyl dithiocarbamate, characterized in that, include: The reactor consists of a first stirring vessel (1), a second stirring vessel (2), a stainless steel high-pressure reactor (3), a rotary evaporator (4), and a vacuum filtration flask (5). A Buchner funnel (6) is provided on the vacuum filtration flask (5). A liquid extraction auxiliary structure is provided between the first stirring vessel (1) and the Buchner funnel (6) on the vacuum filtration flask (5) to assist in introducing the liquid reactants in the first stirring vessel (1) into the Buchner funnel (6) to cooperate with the vacuum filtration flask (5) to perform a reduced pressure filtration operation to produce filtrate. The rotary evaporator (4) is used to evaporate the filtrate to precipitate solids. The second stirring vessel (2) is used to carry out the synthesis reaction of copper dibenzyl dithiocarbamate. The solution after reaction in the second stirring vessel (2) is reacted in the stainless steel high-pressure reactor (3) at a temperature of 80°C for 72 hours.

2. The copper dibenzyl dithiocarbamate synthesis apparatus according to claim 1, characterized in that, The reactants in the first stirring container (1) are magnetically stirred by a magnetic stirrer (7).

3. The copper dibenzyl dithiocarbamate synthesis apparatus according to claim 1, characterized in that, A safety stopcock (8) is provided on the filtration bottle (5) to balance the air pressure inside the filtration bottle (5).

4. The copper dibenzyl dithiocarbamate synthesis apparatus according to claim 1, characterized in that, The filtration flask (5) is evacuated by a vacuum pump (9) to generate negative pressure.

5. The copper dibenzyl dithiocarbamate synthesis apparatus according to claim 1, characterized in that, The liquid extraction auxiliary structure includes a conduit adapter (10), with a first conduit (11) and a second conduit (12) at each end of the conduit adapter (10). The lower end of the conduit adapter (10) is provided with a fixing clamp structure for fixing to the opening position on the first stirring container (1). A support guide tube (13) is provided on one side of the conduit adapter (10). A liquid extraction tube (14) is coaxially inserted in the support guide tube (13). One end of the liquid extraction tube (14) is connected to the first conduit (11), and the other end extends into the support guide tube (13) and slides within the support guide tube (13). The lower end of the liquid extraction tube (14) extends out from the lower end of the support guide tube (13) and into the first stirring container (1). The side surface of the supporting guide tube (13) is provided with a guide opening (15). A slider (16) is provided in the guide opening (15) and connected to the outer surface of the first conduit (11) on the liquid extraction tube (14). The other end of the slider (16) extends out of the supporting guide tube (13) from the guide opening (15). The slider (16) slides in the guide opening (15) and drives the liquid extraction tube (14) to slide in the supporting guide tube (13). The other end of the second conduit (12) is provided with a docking cover (17) communicating with it. The end of the docking cover (17) is provided with a sealing plug (18) inserted into the Buchner funnel (6). The outer side of the sealing plug (18) is sealed with the Buchner funnel (6), and the inner side is connected to the docking cover (17).

6. The copper dibenzyl dithiocarbamate synthesis apparatus according to claim 5, characterized in that, The fixing clamp structure includes a gantry frame (19) fixedly connected to the bottom surface of the lower end of the conduit adapter (10). The gantry frame (19) is used to allow one side wall of the opening position on the first stirring container (1) to extend in. A tightening bolt (20) with a threaded engagement is provided on one side of the gantry frame (19) to fix the gantry frame (19) to the opening position on the first stirring container (1) by pressing it against the outer side wall of the first stirring container (1).

7. The copper dibenzyl dithiocarbamate synthesis apparatus according to claim 1, characterized in that, The stainless steel high-pressure reactor (3) has a polytetrafluoroethylene lining inside.

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